Rapid determination of four components in Jiangzhininggranules by UPLC-MS/MS

摘要：

建立采用超高效液相色谱-串联质谱联用仪(ultra-high performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时快速高效测定降脂宁颗粒中的金丝桃苷、二苯乙烯苷、荷叶碱、橙黄决明素含量的方法.采用Agilent Eclipse Plus C18(2.1 mm×50 mm,1.7μm)色谱柱;流动相是0.05%(体积分数)的甲酸水溶液和0.05%(体积分数)的甲酸-乙腈;流速0.3 mL/min;柱温40℃,进样量5μL;检测时间5 min.电喷雾(electrospray ionization,ESI)离子源,正离子扫描,多反应监测模式(multiple reaction monitoring,MRM).在所设的色谱条件下,5 min内能定量分析出降脂宁颗粒中4种成分,该4种化合物在考察范围内呈良好的线性关系(r≥0.993 6).精密度、稳定性和重复性考察符合分析要求,相对标准偏差(relative standard deviation,RSD)≤4.0%.加标回收率和RSD分别在98.0%~126.9%和0.3%~2.4%范围内.该分析方法简便、快速,灵敏度比较高,专属性强,能在5 min内同时测定降脂宁颗粒中的4种化合物含量,可以为降酯宁颗粒的生产与质量控制提供参考.

Developing a rapid and sensitive method for determining Hyperoside,Tetrahydroxystilbene glucoside,Nuciferine and Aurantio-obtusin in Jiangzhining granules with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The four components of Jiangzhining granules were separated into Agilent Eclipse Plus C 18 column(2.1 mm×50 mm,1.7μm)using 0.05%(volume fraction)formic acid-water(A)and 0.05%(volume fraction)formic acid-Acetonitrile(B)as the mobile phase with gradient elution.The flow rate was 0.3 mL/min and the column temperature was set at 40℃.The injection volume was 5μL,and analysis time was 5 min.The method we used is Electron Spray Ionization(ESI)with positive ion scanning and multiple reaction monitoring(MRM)mode for quantification.Under the optimized chromatographic conditions,four components of the Jiangzhining granules were quantitative analysis within 5 min,and showed a good linear relationship in the range of the study(r≥ 0.9936).It is worth noting that the RSDs of precision,stability and repeatability tests were all no more than 4.0%.The recoveries of four components ranged from 98.0%to 126.9%and RSDs were between 0.3%-2.4%.This method was simple,rapid,specific and accurate within 5 min for the determination of four components in Jiangzhining granules.The current method can be used for the quality control of Jiangzhining granules.

作者：

刘慢 余文洁 赵新娜 陈昱安 赵阗 张晓凡

Liu Man;Yu Wenjie;Zhao Xinna;Chen Yuan;Zhao Tian;Zhang Xiaofan(Henan Key Laboratory of Nanocomposites and Applications,Huanghe Science and Technology College,Zhengzhou 450052,China;Henan Environment Monitoring Center,Zhengzhou 450004,China;School of Materials Science and Engineering,Dongguan University of Technology,Dongguan 523808,China)

机构地区：

黄河科技学院河南省纳米复合材料与应用重点实验室 河南省环境监测中心 东莞理工学院材料科学与工程学院

出处：

《betway官方app 学报：自然科学版》 CAS 北大核心 2020年第5期74-79,共6页

基金：

国家自然科学基金(51602120) 东莞理工学院科研启动专项经费项目(GC300501-126).

关键词：

超高效液相色谱-串联质谱法 降脂宁颗粒 快速检测 多反应监测模式

UPLC-MS/MS Jiangzhining granules rapid determination multiple reaction monitoring

分类号：

O657.63 [理学—分析化学]

UPLC-MS_MS法快速测定降脂宁颗粒中4种化合物的含量.pdf